CN113501991A - Formula, preparation method and production equipment of high-tensile-strength PBT material - Google Patents
Formula, preparation method and production equipment of high-tensile-strength PBT material Download PDFInfo
- Publication number
- CN113501991A CN113501991A CN202110889077.9A CN202110889077A CN113501991A CN 113501991 A CN113501991 A CN 113501991A CN 202110889077 A CN202110889077 A CN 202110889077A CN 113501991 A CN113501991 A CN 113501991A
- Authority
- CN
- China
- Prior art keywords
- pbt
- pbt material
- preparation
- carbon fiber
- tensile
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/046—Forming abrasion-resistant coatings; Forming surface-hardening coatings
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/02—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type
- B29B7/06—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices
- B29B7/10—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices rotary
- B29B7/12—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices rotary with single shaft
- B29B7/16—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices rotary with single shaft with paddles or arms
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/80—Component parts, details or accessories; Auxiliary operations
- B29B7/82—Heating or cooling
- B29B7/826—Apparatus therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/80—Component parts, details or accessories; Auxiliary operations
- B29B7/84—Venting or degassing ; Removing liquids, e.g. by evaporating components
- B29B7/845—Venting, degassing or removing evaporated components in devices with rotary stirrers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/80—Component parts, details or accessories; Auxiliary operations
- B29B7/86—Component parts, details or accessories; Auxiliary operations for working at sub- or superatmospheric pressure
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/0405—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
- C08J5/042—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres with carbon fibres
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/0427—Coating with only one layer of a composition containing a polymer binder
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/544—Silicon-containing compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a formula, a preparation method and production equipment of a high tensile strength PBT material, which comprises the following steps: s1: carrying out ester exchange reaction on 1, 4-butanediol and terephthalic acid diformate to generate dibutyl terephthalate, removing methanol, and carrying out polycondensation reaction to produce a PBT resin raw material; s2: the method comprises the following steps of: 45-50 parts of PBT resin raw material, 0.3-0.7 part of acrylic polymer chain extender ADR, 0.3-0.8 part of coupling agent and 0.02-0.04 part of antioxidant are added into PBT material production equipment, and the PBT material is preheated to control the temperature to 230-240 ℃ and is continuously stirred. According to the invention, the carbon fiber is added into the PBT material for treatment, and the coupling agent is utilized for mixing and kneading the PBT material and the carbon fiber, so that the wettability of the carbon fiber short branches in the PBT resin is improved, the compatibility of the PBT resin and the carbon fiber short branches is increased, the mechanical property of the composite material is improved, and the composite material has the advantages of high temperature resistance, high tensile strength, high bending strength, high tensile strength and the like, and the physical and chemical properties of the PBT material are improved.
Description
Technical Field
The invention relates to the technical field of PBT materials, in particular to a formula, a preparation method and production equipment of a high-tensile PBT material.
Background
Polybutylene terephthalate (PBT) is a colorless and transparent thermoplastic resin, and is widely used because it is inexpensive and easy to process. Wollastonite is a triclinic system, fine tabular crystal has low oil absorption, low conductivity and good insulation property, and is mainly used as a reinforcing filler of a high polymer-based composite material. Polybutylene terephthalate (PBT) has excellent fluidity, chemical resistance and heat resistance, and carbon fiber has the characteristics of high temperature resistance, high strength, high modulus, corrosion resistance, fatigue resistance and the like, is a novel fiber material with light weight and high strength, is mainly used for preparing advanced composite materials, and is widely applied to the fields of aerospace, automobiles, wind power blades, sports and leisure and the like.
Polybutylene terephthalate (PBT) is one of five engineering plastics, and has the characteristics of high crystallization speed, excellent electrical property, good chemical resistance, excellent mechanical property and outstanding friction resistance and abrasion resistance, but the PBT has the defects of poor dimensional stability, low notch impact strength and the like, so that the application of the PBT is limited. ABS resin (acrylonitrile-butadiene-styrene copolymer) is the plastic with the largest output and the most extensive application at present, the price is cheaper, ABS not only has mechanical properties of toughness, hardness and rigidity in balance, but also has better dimensional stability, surface gloss, low temperature resistance, coloring processability and processing fluidity, so that PBT and ABS are blended to prepare plastic alloy with excellent performance, and the high performance of the resin is realized.
The tensile resistance means that when the PBT material is assembled, one end of the PBT material sheet needs to be embedded into a drawing clamp, then, the insert is pulled out by a tensile tester, the measured force is tensile resistance, the tensile resistance is the structural strength of the PBT material sheet, the higher the tensile resistance is, the better the property of the PBT material is, the test shows that the existing common PBT material does not mention the relevant test of the tensile force in the tensile effect, the tensile property of the PBT material is weaker, in some specific use occasions, such as a wiring terminal insulating base and a vehicle part scene, the service life is short, certain defects exist, in view of the above, research and improvement are carried out on the existing problems, and a formula, a preparation method and production equipment of a high-tensile-strength PBT material are provided, so that the problems of insufficient tensile strength and small application range existing at present are solved, and the purposes of solving the problems and improving the practical value are achieved through the technology.
Disclosure of Invention
The present invention is directed to solving one of the technical problems of the prior art or the related art.
Therefore, the technical scheme adopted by the invention is as follows: a formula and a preparation method of a high-tensile PBT material comprise the following steps: s1: carrying out ester exchange reaction on 1, 4-butanediol and terephthalic acid diformate to generate dibutyl terephthalate, removing methanol, and carrying out polycondensation reaction to produce a PBT resin raw material;
s2: the method comprises the following steps of: 45-50 parts of PBT resin raw material, 0.3-0.7 part of acrylic polymer chain extender ADR, 0.3-0.8 part of coupling agent and 0.02-0.04 part of antioxidant are added into production equipment of PBT material, the PBT resin is preheated to control the temperature to 230-240 ℃ and is continuously stirred, the coupling agent is one or a combination of more of aminopropyltriethoxysilane KH-550, methacryloxy and titanate coupling agent 101, and the antioxidant is hindered phenol antioxidant 1010 and phosphite antioxidant 626, and the mass components are as follows: 1.2 mixing the mixture;
s3: the pressurizing interface of the device is communicated with a compression pump, nitrogen is introduced to pressurize the interior of the reaction device, the air pressure of the inner cavity of the device is kept at 0.5-0.6MPa, and the duration is 15-20 min;
s4: injecting 10-13 parts of carbon fiber into a product obtained after reaction, dehydration and drying according to the mass fraction ratio, adding the product into a double-screw extruder for extrusion through respective precisely metered feeders, wherein the carbon fiber is in a short fiber structure with the length of 12-20nm, carrying out oxidation calcination treatment at the temperature of 480 ℃ for 5-30min, sequentially treating the carbon fiber with acid and alkali to make the carbon fiber neutral, then drying the treated carbon fiber, and carrying out injection molding and temperature control on the carbon fiber at the front stage: 245-270 ℃, middle section: 240-250 ℃, and the rear section: 230-240 ℃, nozzle: 250-270 ℃, mold temperature: 30-80 ℃, injection molding pressure: 500-1000 kg/cm2, screw rotation speed: obtaining a product at 40-100 rpm;
s5: and (3) immediately spraying an auxiliary agent on the surface of the product after demoulding, wherein the auxiliary agent is a UV coating and comprises an active diluent monomer, oligomeric resin, a photoinitiator, a second adhesion promoter and a diluent, heating the auxiliary agent by using the residual demoulding temperature of the product, and irradiating and curing by using ultraviolet light.
Further, in the step S2, the following raw materials are used in mass fraction: 45-50 parts of PBT resin raw material, 0.7-0.9 part of acrylic polymer chain extender ADR, 0.8-1.0 part of coupling agent and 0.02-0.04 part of antioxidant are added into PBT material production equipment, and the PBT material is preheated to control the temperature to 230-240 ℃ and is continuously stirred.
A production facility of high tensile PBT material includes: preparation jar and stirring actuating mechanism, the sleeve seat has been cup jointed in the bottom activity of preparation jar, the top surface of preparation jar is equipped with sealed pressure retaining cover, stirring actuating mechanism's underrun sealed pressure retaining cover and the top sealing connection of preparation jar, the outside of preparation jar is fixed to be cup jointed and is located the inside eddy current heating coil of sleeve seat, the bottom surface fixedly connected with return bend of unloading of preparation jar, stirring actuating mechanism includes driving motor, motion air intake dish, puddler and aeration dispersion mechanism, driving motor's output is through the motion air intake dish and the top fixed connection of puddler, aeration dispersion mechanism fixed mounting is in the one end of puddler.
The present invention in a preferred example may be further configured to: the stirring rod is of a round tubular long rod structure, a plurality of air inlet grooves are formed in the peripheral side of the movement rotating wheel and communicated with the inner cavity of the stirring rod, and an air inlet hole is formed in one side of the movement air inlet disc.
Through adopting above-mentioned technical scheme, in the rotation of puddler, connect the inside that the motion air inlet dish was gone into the preparation jar with the protector pressurization pump through high-pressure air pump, carry out high temperature pressurization to the material and handle, utilize high pressure to carry out PBT material high pressure and remove bubble processing and discharge the bubble in the interior a large amount of fine clearance holes of PBT, improve the structural compactness of PBT material and further improve the structural strength of PBT material.
The present invention in a preferred example may be further configured to: the surface of the aeration dispersion mechanism is provided with a plurality of air outlets, the inside of the aeration dispersion mechanism is rotatably provided with an aeration turbine, and the bottom end of the stirring rod is communicated with the inside of the aeration dispersion mechanism.
Through adopting above-mentioned technical scheme, at the in-process that the puddler admitted air, gaseous promotion aeration turbine carries out rotary motion to it releases to aerate to admit air through aeration turbine reverse promotion, and the inside bubble that produces of PBT material is avoided in the pressurization of evenly giving vent to anger.
The beneficial effects obtained by the invention are as follows:
1. according to the invention, the carbon fiber is added into the PBT material for treatment, and the coupling agent is utilized for mixing and kneading the PBT material and the carbon fiber, so that the wettability of the carbon fiber short branches in the PBT resin is improved, the compatibility of the PBT resin and the carbon fiber short branches is increased, the mechanical property of the composite material is improved, and the composite material has the advantages of high temperature resistance, high tensile strength, high bending strength, high tensile strength and the like, and the physical and chemical properties of the PBT material are improved.
2. According to the invention, the surface of the PBT material is subjected to auxiliary agent spraying and UV photocuring treatment, and a layer of UV-curable coating is coated and cured to form the UV-curable coating, so that the nanometer defects formed on the surface of the cross-linked mixed material of the carbon fiber and the PBT material are repaired, and the hardness and the wear resistance of the surface of the PBT material are improved.
3. According to the invention, high-tightness stirring preparation equipment is adopted, the material mixing and heating are carried out in an integrated operation mode, the protection gas pressurization operation is carried out in the preparation process, high-pressure bubble removal treatment is carried out on the PBT material under high pressure, bubbles in a large number of fine-gap holes in the PBT material are discharged, the structural compactness of the PBT material is improved, and the structural strength of the PBT material is further improved.
Drawings
FIG. 1 is a schematic overall structure diagram of one embodiment of the present invention;
FIG. 2 is a schematic view of an agitation drive mechanism according to one embodiment of the present invention;
FIG. 3 is a schematic diagram of a preparation tank according to one embodiment of the present invention;
FIG. 4 is a schematic view of the internal structure of a moving intake plate according to an embodiment of the present invention;
fig. 5 is a schematic structural view of an aeration dispersing mechanism according to an embodiment of the present invention.
Reference numerals:
100. preparing a tank; 110. a sleeve seat; 120. a sealing and pressure-maintaining cover; 130. discharging a bent pipe; 140. an eddy current heating coil;
200. a stirring drive mechanism; 210. a drive motor; 220. a motion air intake disc; 230. a stirring rod; (ii) a 240. An aeration dispersion mechanism; 231. a motion runner; 232. an air inlet groove; (ii) a 241. An aeration turbine.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings in conjunction with the following detailed description. It should be noted that the embodiments of the present invention and features of the embodiments may be combined with each other without conflict.
It is to be understood that this description is made only by way of example and not as a limitation on the scope of the invention.
The following describes the formula, preparation method and production equipment of a high-tensile PBT material provided by some embodiments of the invention with reference to the accompanying drawings.
Example 1:
with reference to fig. 1 to 5, the formula and the preparation method of the high tensile strength PBT material provided by the invention comprise the following steps: s1: carrying out ester exchange reaction on 1, 4-butanediol and terephthalic acid diformate to generate dibutyl terephthalate, removing methanol, and carrying out polycondensation reaction to produce a PBT resin raw material;
s2: the method comprises the following steps of: 45-50 parts of PBT resin raw material, 0.3-0.7 part of acrylic polymer chain extender ADR, 0.3-0.8 part of coupling agent and 0.02-0.04 part of antioxidant are added into production equipment of PBT material, the PBT material is preheated to be controlled to 230-240 ℃ and is continuously stirred, the coupling agent is one or more of aminopropyltriethoxysilane KH-550, methacryloxy and titanate coupling agent 101, and the antioxidant is hindered phenol antioxidant 1010 and phosphite antioxidant 626, and the mass components are as follows: 1.2 mixing the mixture;
s3: the pressurizing interface of the device is communicated with a compression pump, nitrogen is introduced to pressurize the interior of the reaction device, the air pressure of the inner cavity of the device is kept at 0.5-0.6MPa, and the duration is 15-20 min;
s4: injecting 10-13 parts of carbon fiber into a product obtained after reaction, dehydration and drying according to the mass fraction ratio, adding the product into a double-screw extruder for extrusion through respective precisely metered feeders, wherein the carbon fiber is in a short fiber structure with the length of 12-20nm, carrying out oxidation calcination treatment at the temperature of 480 ℃ for 5-30min, sequentially treating the carbon fiber with acid and alkali to make the carbon fiber neutral, then drying the treated carbon fiber, and carrying out injection molding and temperature control on the carbon fiber at the front stage: 245-270 ℃, middle section: 240-250 ℃, and the rear section: 230-240 ℃, nozzle: 250-270 ℃, mold temperature: 30-80 ℃, injection molding pressure: 500-1000 kg/cm2, screw rotation speed: obtaining a product at 40-100 rpm;
s5: and (3) immediately spraying an auxiliary agent on the surface of the product after demoulding, wherein the auxiliary agent is a UV coating and comprises an active diluent monomer, oligomeric resin, a photoinitiator, a second adhesion promoter and a diluent, heating the auxiliary agent by using the residual demoulding temperature of the product, and irradiating and curing by using ultraviolet light.
The UV coating is characterized by comprising the following components in percentage by mass, wherein the content of the reactive diluent monomer is preferably 1.0-2%; the content of the oligomeric resin is preferably 30-40%; the content of the photoinitiator is preferably 0.8-1.6%; the content of the second adhesion promoter is preferably 0.5-2%; the content of the diluent is preferably 40-50%;
in this embodiment, the oligomeric resin is a silicone resin and a 4-6 functional urethane acrylate, which may be selected from one or more of CN990, CN9006, and 1700B, the photoinitiator is a photoinitiator in the prior art, which may be selected from one or two of photoinitiators 1173 and 184, and the second adhesion promoter is an aminosilane compound, which is commonly known to those skilled in the art, and may be one of dele 1121, american carbon a-1100, and JH-a110 of jianghan fine chemical company, for example.
A production facility of high tensile PBT material includes: the bottom end of the preparation tank 100 is movably sleeved with a sleeve seat 110, the top surface of the preparation tank 100 is provided with a sealing and pressure-maintaining cover 120, the bottom surface of the stirring driving mechanism 200 is connected with the top end of the preparation tank 100 through the sealing and pressure-maintaining cover 120 in a sealing manner, the outer side of the preparation tank 100 is fixedly sleeved with a vortex heating coil 140 positioned inside the sleeve seat 110, the bottom surface of the preparation tank 100 is fixedly connected with a discharge elbow 130, the stirring driving mechanism 200 comprises a driving motor 210, a motion air inlet disc 220, a stirring rod 230 and an aeration dispersion mechanism 240, the output end of the driving motor 210 is fixedly connected with the top end of the stirring rod 230 through the motion air inlet disc 220, and the aeration dispersion mechanism 240 is fixedly installed at one end of the stirring rod 230.
In this embodiment, a moving rotating wheel 231 is rotatably installed inside the moving air intake disc 220, the stirring rod 230 is a round tubular long rod structure, a plurality of air intake slots 232 are formed on the periphery side of the moving rotating wheel 231, the air intake slots 232 are communicated with the inner cavity of the stirring rod 230, and an air intake hole is formed on one side of the moving air intake disc 220.
Specifically, during the rotation of the stirring rod 230, the high-pressure air pump is connected with the moving air inlet disc 220 to pump the protector into the preparation tank 100 in a pressurizing manner, the materials are subjected to high-temperature pressurizing treatment, and high-pressure defoaming treatment of the PBT materials is performed under high pressure to discharge air bubbles in a large number of fine gap holes in the PBT materials, so that the structural compactness of the PBT materials is improved, and the structural strength of the PBT materials is further improved.
In this embodiment, a plurality of air outlet holes are formed on the surface of the aeration dispersing mechanism 240, an aeration turbine 241 is rotatably installed inside the aeration dispersing mechanism 240, the bottom end of the stirring rod 230 is communicated with the inside of the aeration dispersing mechanism 240, and in the air inlet process of the stirring rod 230, the air pushes the aeration turbine 241 to rotate, so that the aeration turbine 241 reversely pushes the inlet air to be dispersed and pushed out, and air is uniformly discharged and pressurized to avoid bubbles inside the PBT material.
Example 2:
the difference from example 1 is that S1: carrying out ester exchange reaction on 1, 4-butanediol and terephthalic acid diformate to generate dibutyl terephthalate, removing methanol, and carrying out polycondensation reaction to produce a PBT resin raw material;
s2: the method comprises the following steps of: 45-50 parts of PBT resin raw material, 0.7-0.9 part of acrylic polymer chain extender ADR, 0.8-1.0 part of coupling agent and 0.02-0.04 part of antioxidant are added into production equipment of PBT material, the PBT material is preheated to be controlled to 230-240 ℃ and is continuously stirred, the coupling agent is one or a combination of more of aminopropyltriethoxysilane KH-550, methacryloxy and titanate coupling agent 101, and the antioxidant is hindered phenol antioxidant 1010 and phosphite antioxidant 626, and the mass components are as follows: 1.2 mixing the mixture;
s3: the pressurizing interface of the device is communicated with a compression pump, nitrogen is introduced to pressurize the interior of the reaction device, the air pressure of the inner cavity of the device is kept at 0.5-0.6MPa, and the duration is 15-20 min;
s4: injecting 10-13 parts of carbon fiber into a product obtained after reaction, dehydration and drying according to the mass fraction ratio, adding the product into a double-screw extruder for extrusion through respective precisely metered feeders, wherein the carbon fiber is in a short fiber structure with the length of 12-20nm, carrying out oxidation calcination treatment at the temperature of 480 ℃ for 5-30min, sequentially treating the carbon fiber with acid and alkali to make the carbon fiber neutral, then drying the treated carbon fiber, and carrying out injection molding and temperature control on the carbon fiber at the front stage: 245-270 ℃, middle section: 240-250 ℃, and the rear section: 230-240 ℃, nozzle: 250-270 ℃, mold temperature: 30-80 ℃, injection molding pressure: 500-1000 kg/cm2, screw rotation speed: obtaining a product at 40-100 rpm;
s5: and (3) immediately spraying an auxiliary agent on the surface of the product after demoulding, wherein the auxiliary agent is a UV coating and comprises an active diluent monomer, oligomeric resin, a photoinitiator, a second adhesion promoter and a diluent, heating the auxiliary agent by using the residual demoulding temperature of the product, and irradiating and curing by using ultraviolet light.
The advantages of this embodiment are: by increasing the content ratio of the coupling agent to the chain extender, the graft capacity of the PBT resin raw material is improved, the grafting effect with the carbon fiber is increased, and a large number of anti-tensile fiber structures are mixed, so that the mechanical property of the composite material is improved, the advantages of high temperature resistance, high tensile strength, high bending strength, high tensile strength and the like are further improved, and the physical and chemical properties of the PBT material are improved.
In the present invention, the term "plurality" means two or more unless explicitly defined otherwise. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items. The terms "mounted," "connected," "fixed," and the like are used broadly and encompass, for example, a fixed connection, a removable connection, or an integral connection, and a connection may be a direct connection or an indirect connection via intermediate media. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
It will be understood that when an element is referred to as being "mounted to," "secured to" or "disposed on" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. The terms "vertical," "horizontal," "upper," "lower," "left," "right," and the like as used herein are for illustrative purposes only and do not denote a unique embodiment.
In the description herein, the description of the terms "one embodiment," "some embodiments," "specific embodiments," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the claims and their equivalents.
Claims (9)
1. The formula and the preparation method of the high-tensile-strength PBT material are characterized by comprising the following steps of:
s1: carrying out ester exchange reaction on 1, 4-butanediol and terephthalic acid diformate to generate dibutyl terephthalate, removing methanol, and carrying out polycondensation reaction to produce a PBT resin raw material;
s2: the method comprises the following steps of: 45-50 parts of PBT resin raw material, 0.3-0.7 part of acrylic polymer chain extender ADR, 0.3-0.8 part of coupling agent and 0.02-0.04 part of antioxidant are added into PBT material production equipment, preheated to control the temperature to 230-240 ℃ and continuously stirred;
s3: the pressurizing interface of the device is communicated with a compression pump, nitrogen is introduced to pressurize the interior of the reaction device, the air pressure of the inner cavity of the device is kept at 0.5-0.6MPa, and the duration is 15-20 min;
s4: injecting 10-13 parts of carbon fiber into the product after reaction, dehydration and drying according to the mass fraction ratio, adding the product into a double-screw extruder through respective precisely-metered feeders, and extruding, wherein the injection molding temperature control front section comprises the following steps: 245-270 ℃, middle section: 240-250 ℃, and the rear section: 230-240 ℃, nozzle: 250-270 ℃, mold temperature: 30-80 ℃, injection molding pressure: 500-1000 kg/cm2, screw rotation speed: obtaining a product at 40-100 rpm;
s5: and (3) immediately spraying an auxiliary agent on the surface of the product after demoulding, heating the auxiliary agent by using the residual demoulding temperature of the product, and irradiating and curing by using ultraviolet light.
2. The formula and the preparation method of the high-tensile PBT material according to claim 1, wherein in step S2, the following raw materials are used in mass fraction: 45-50 parts of PBT resin raw material, 0.7-0.9 part of acrylic polymer chain extender ADR, 0.8-1.0 part of coupling agent and 0.02-0.04 part of antioxidant are added into PBT material production equipment, and the PBT material is preheated to control the temperature to 230-240 ℃ and is continuously stirred.
3. The formulation and the preparation method of a high tensile strength PBT material according to claim 1 or 2, characterized in that the coupling agent is one or more of aminopropyltriethoxysilane KH-550, methacryloxy and titanate coupling agent 101.
4. The formula and the preparation method of the high-tensile-strength PBT material according to claim 1 or 2, wherein the antioxidant is a hindered phenol antioxidant 1010 and a phosphite antioxidant 626, and the mass components are as follows: 1.2 compounding.
5. The formula and the preparation method of the high tensile PBT material according to claim 1, wherein in step S4, the carbon fiber is a short fiber structure with a length of 12-20nm, and is subjected to an oxidizing calcination treatment at 480 ℃ for 5-30min, and then to a neutralization treatment by sequentially using an acid and an alkali, and then the treated carbon fiber is dried.
6. The formulation and the preparation method of a high tensile PBT material according to claim 1, wherein in the step S5, the auxiliary agent is a UV coating comprising a reactive diluent monomer, an oligomeric resin, a photoinitiator, a second adhesion promoter and a diluent.
7. Production facility of high tensile PBT material which characterized in that includes: a preparation tank (100) and a stirring driving mechanism (200), wherein the bottom end of the preparation tank (100) is movably sleeved with a sleeve seat (110), the top surface of the preparation tank (100) is provided with a sealing and pressure-maintaining cover (120), the bottom surface of the stirring driving mechanism (200) is hermetically connected with the top end of the preparation tank (100) through the sealing and pressure-maintaining cover (120), the outer side of the preparation tank (100) is fixedly sleeved with a vortex heating coil (140) positioned in the sleeve seat (110), the bottom surface of the preparation tank (100) is fixedly connected with a discharge elbow (130), the stirring driving mechanism (200) comprises a driving motor (210), a moving air inlet disc (220), a stirring rod (230) and an aeration dispersion mechanism (240), the output end of the driving motor (210) is fixedly connected with the top end of the stirring rod (230) through a moving air inlet disc (220), the aeration dispersion mechanism (240) is fixedly arranged at one end of the stirring rod (230).
8. The production equipment of the high tensile PBT material according to claim 7, wherein a moving rotating wheel (231) is rotatably installed inside the moving air inlet disc (220), the stirring rod (230) is a round tubular long rod structure, a plurality of air inlet grooves (232) are formed in the periphery of the moving rotating wheel (231), the air inlet grooves (232) are communicated with the inner cavity of the stirring rod (230), and an air inlet hole is formed in one side of the moving air inlet disc (220).
9. The production equipment of the high tensile PBT material according to claim 7, wherein a plurality of air outlets are opened on the surface of the aeration dispersion mechanism (240), an aeration turbine (241) is rotatably installed inside the aeration dispersion mechanism (240), and the bottom end of the stirring rod (230) is communicated with the inside of the aeration dispersion mechanism (240).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110889077.9A CN113501991A (en) | 2021-08-04 | 2021-08-04 | Formula, preparation method and production equipment of high-tensile-strength PBT material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110889077.9A CN113501991A (en) | 2021-08-04 | 2021-08-04 | Formula, preparation method and production equipment of high-tensile-strength PBT material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113501991A true CN113501991A (en) | 2021-10-15 |
Family
ID=78014993
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110889077.9A Pending CN113501991A (en) | 2021-08-04 | 2021-08-04 | Formula, preparation method and production equipment of high-tensile-strength PBT material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113501991A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102236113A (en) * | 2010-05-01 | 2011-11-09 | 中国航天科技集团公司第四研究院第四十二所 | Ultraviolet-cured hard coating and application thereof |
| CN102963106A (en) * | 2012-12-07 | 2013-03-13 | 深圳市志凌伟业技术有限公司 | High-pressure bubble removing method for capacitive touch screen |
| CN104194286A (en) * | 2014-08-13 | 2014-12-10 | 上海交通大学 | Carbon fiber reinforced thermoplastic resin composite material and preparation method of carbon fiber reinforced thermoplastic resin composite material |
| US20180016420A1 (en) * | 2015-01-25 | 2018-01-18 | Ftex Incorporated | Method for producing modified polyester resin reinforced with carbon fiber |
| CN107698956A (en) * | 2017-10-23 | 2018-02-16 | 深圳市京信通科技有限公司 | Fibre reinforced PC/PBT alloys of surface treatment and preparation method thereof |
| CN212882211U (en) * | 2020-07-30 | 2021-04-06 | 广州文晖医药科技有限公司 | Raw materials compounding equipment of chemical reagent |
-
2021
- 2021-08-04 CN CN202110889077.9A patent/CN113501991A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102236113A (en) * | 2010-05-01 | 2011-11-09 | 中国航天科技集团公司第四研究院第四十二所 | Ultraviolet-cured hard coating and application thereof |
| CN102963106A (en) * | 2012-12-07 | 2013-03-13 | 深圳市志凌伟业技术有限公司 | High-pressure bubble removing method for capacitive touch screen |
| CN104194286A (en) * | 2014-08-13 | 2014-12-10 | 上海交通大学 | Carbon fiber reinforced thermoplastic resin composite material and preparation method of carbon fiber reinforced thermoplastic resin composite material |
| US20180016420A1 (en) * | 2015-01-25 | 2018-01-18 | Ftex Incorporated | Method for producing modified polyester resin reinforced with carbon fiber |
| CN107698956A (en) * | 2017-10-23 | 2018-02-16 | 深圳市京信通科技有限公司 | Fibre reinforced PC/PBT alloys of surface treatment and preparation method thereof |
| CN212882211U (en) * | 2020-07-30 | 2021-04-06 | 广州文晖医药科技有限公司 | Raw materials compounding equipment of chemical reagent |
Non-Patent Citations (1)
| Title |
|---|
| 杨卫民: "滚塑中气泡的消除", 《2015中国国际滚塑论坛论文集》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103154140B (en) | Method for producing thermoplastic resin composition, thermoplastic resin composition, and molded product | |
| CN103849018B (en) | Rice hull ash/macromolecular composite material, preparation method and application thereof | |
| Kuan et al. | Mechanical, thermal and morphological properties of water-crosslinked wood flour reinforced linear low-density polyethylene composites | |
| CN101792596A (en) | Composite material for recycling waste vehicle nylon products and preparation method thereof | |
| WO2019127417A1 (en) | High-strength and easy-to-electroplate polyamide composite material and preparation method therefor | |
| CN107892772A (en) | A kind of lightweight that resist warping continuous glass-fiber reinforced polypropylene compound material and preparation method | |
| JPH0618929B2 (en) | Glass fiber reinforced polypropylene composition | |
| CN111548600A (en) | Modified carbon fiber reinforced thermoplastic resin composite material | |
| CN102863785A (en) | Enhanced polyamide compound and preparation method thereof | |
| CN109627759A (en) | A kind of PA66 reinforcing material and its preparation method and application | |
| CN109081894B (en) | High-fluidity toughening agent and preparation method thereof | |
| CN114207027A (en) | Liquid crystal polyester resin pellet, process for producing the same, and process for producing molded article | |
| CN105482355A (en) | Reinforcing and toughening agent for 3D printing of ABS and ABS composite | |
| CN105623250A (en) | Polyamide, glass fiber and interface bonding agent composite and preparation method thereof | |
| CN113501991A (en) | Formula, preparation method and production equipment of high-tensile-strength PBT material | |
| CN105837806A (en) | Liquid crystal polyester and its molded composition and use | |
| US5534302A (en) | Method of preparing a fiber reinforced modified phenolic resin composite | |
| CN111548624A (en) | High-strength MC nylon 6-based composite material and preparation method thereof | |
| CN111073203A (en) | Continuous long glass fiber modified polypropylene composite material and preparation method thereof | |
| CN114369352A (en) | High-toughness heat-conducting PC composite material and preparation method thereof | |
| CN112029271A (en) | Spraying-free polycaprolactam composite material and preparation method thereof | |
| CN114207026A (en) | Liquid crystal polyester resin molded article | |
| CN114806154B (en) | Highlight black composite nylon material and preparation method and application thereof | |
| CN115340728B (en) | Scratch-resistant polypropylene resin material | |
| JPH0236244A (en) | Thermoplastic resin composition |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20211015 |
|
| RJ01 | Rejection of invention patent application after publication |